CN104000854A - Pretreatment method for preparing phellinus igniarius functional component - Google Patents
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- CN104000854A CN104000854A CN201410233913.8A CN201410233913A CN104000854A CN 104000854 A CN104000854 A CN 104000854A CN 201410233913 A CN201410233913 A CN 201410233913A CN 104000854 A CN104000854 A CN 104000854A
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- 241000123113 Phellinus igniarius Species 0.000 title claims abstract description 60
- 238000002203 pretreatment Methods 0.000 title abstract 2
- 239000000843 powder Substances 0.000 claims abstract description 43
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 16
- 239000003513 alkali Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000001125 extrusion Methods 0.000 claims abstract description 10
- 239000002245 particle Substances 0.000 claims abstract description 9
- 238000010298 pulverizing process Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- 238000001238 wet grinding Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 239000000284 extract Substances 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 3
- 230000001276 controlling effect Effects 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims 1
- 238000000605 extraction Methods 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 7
- 239000007787 solid Substances 0.000 abstract 3
- 239000008187 granular material Substances 0.000 description 7
- 150000004676 glycans Chemical class 0.000 description 6
- 229920001282 polysaccharide Polymers 0.000 description 6
- 239000005017 polysaccharide Substances 0.000 description 6
- 210000004027 cell Anatomy 0.000 description 5
- 210000002421 cell wall Anatomy 0.000 description 5
- 229920002101 Chitin Polymers 0.000 description 4
- 238000004626 scanning electron microscopy Methods 0.000 description 4
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 3
- 229930003944 flavone Natural products 0.000 description 3
- 150000002212 flavone derivatives Chemical class 0.000 description 3
- 235000011949 flavones Nutrition 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 230000003834 intracellular effect Effects 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 150000008442 polyphenolic compounds Chemical class 0.000 description 2
- 235000013824 polyphenols Nutrition 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000008234 soft water Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 241000222382 Agaricomycotina Species 0.000 description 1
- 229920001661 Chitosan Polymers 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 229920001503 Glucan Polymers 0.000 description 1
- 229920000057 Mannan Polymers 0.000 description 1
- 241001597008 Nomeidae Species 0.000 description 1
- 241000123107 Phellinus Species 0.000 description 1
- 241000222341 Polyporaceae Species 0.000 description 1
- 241000222383 Polyporales Species 0.000 description 1
- 241001072909 Salvia Species 0.000 description 1
- 235000017276 Salvia Nutrition 0.000 description 1
- 229930183415 Suberin Natural products 0.000 description 1
- 241000001727 Tropicoporus linteus Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 239000002246 antineoplastic agent Substances 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000002538 fungal effect Effects 0.000 description 1
- 150000002402 hexoses Chemical class 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- TWNIBLMWSKIRAT-VFUOTHLCSA-N levoglucosan Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@H]2CO[C@@H]1O2 TWNIBLMWSKIRAT-VFUOTHLCSA-N 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000011275 oncology therapy Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000008104 plant cellulose Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 230000008542 thermal sensitivity Effects 0.000 description 1
- 150000003648 triterpenes Chemical class 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
Abstract
The invention provides a pretreatment method for preparing a phellinus igniarius functional component, which relates to the technology of medium-temperature dual-screw extrusion and alkali treatment. The method relates to the technology of phellinus igniarius solid dual-screw extrusion and alkali treatment wall breaking technology, the prepared phellinus igniarius powder is high in cell disruption degree and loose in structure, and extraction of the phellinus igniarius functional component is facilitated. The temperature of a cutting area and the terminal of an extruder is controlled to be 60-80 DEG C, the phellinus igniarius solid fine powder subjected to dual-screw extruding crushing is adopted, the diameter of the uniform particles is remarkably smaller than 100 mu m, and the cells can be disrupted completed; the obtained phellinus igniarius solid fine powder is treated for 5 hours by 0.6mol/L NaOH which is five times the amount of the fine powder, so that the extraction yield of the functional component can be remarkably improved to 153-276 percent.
Description
Technical field
The present invention relates to pre-treating method prepared by a kind of Phellinus igniarius (L. ex Fr.) Quel. functional component, by middle temperature twin screw extruding combined alkali treatment technology, realize.
Background technology
Phellinus igniarius (L. ex Fr.) Quel.
(Phellinus Linteus)-belong to Basidiomycotina, Hymenomycetes, Aphyllophorales, Polyporaceae, Phellinus, is the generally acknowledged higher a kind of large-scale medicinal fungi of active anticancer of biological field of finding at present.The existing people of Japan makes anti-tumor agent the extract of Phellinus igniarius (L. ex Fr.) Quel., and has applied for patent.Korea S was successfully developed to cancer therapy drug by Phellinus igniarius (L. ex Fr.) Quel. in 1993.In recent years, Korea S, Japan, China and more American-European countries are all in the exploitation dynamics strengthening Phellinus igniarius (L. ex Fr.) Quel. medicine.
Natural Phellinus igniarius (L. ex Fr.) Quel. sporophore is perennial, the hard and lignifying of cap, and bacterial context is generally soft suberin or hard wooden.General fungal cell's wall thickness is 100～250nm approximately, and it accounts for cell dry approximately 30%～60%.Cell wall mainly contains chitin (chitin), cellulose, glucosan, mannan isostructuralism composition of Salvia polysaccharide.Chitin is a kind of macromolecule polysaccharide of line style, and chitinous chemical constitution and plant cellulose are closely similar, is all the polymer of hexose, and molecular weight is all more than 1,000,000, and the ultimate unit of chitosan is glucamine.Chitin is water insoluble, diluted acid, alkali, ethanol or other organic solvent.Because Phellinus igniarius (L. ex Fr.) Quel. sporophore structure is hard, fine and close, Ordinary pulverization is difficult to make its cell rupture, has affected the leaching of Phellinus igniarius (L. ex Fr.) Quel. functional components (polysaccharide, flavone and derivant thereof and triterpene substance).
In During Screw Extrusion, mainly utilize twin screw to effects such as the extruding of material, friction, shearings, control water content, the main frame temperature of material simultaneously well, when making material grind carefullyyer, the loss that also can avoid the degraded of heat-sensitive substance to bring.
Alkali treatment method is first to add certain density alkali before extracting by material, and under proper condition, alkali can be partly dissolved soluble polysaccharide layer and the lipid of material cell, thereby makes the permeability of cell wall become large, and intracellular organic matter is easy to separate out.By controlling temperature and time, avoid violent processing, both made cell wall breaking, intracellular organic matter is discharged to greatest extent, does not cause the hydrolysis of functional materials again and loses.
Summary of the invention
The object of the invention is to apply Twin-Screw Extrusion Technology Phellinus igniarius (L. ex Fr.) Quel. sporophore is carried out to extrusion breaking cellular wall; gained Phellinus igniarius (L. ex Fr.) Quel. sporophore fine powder cell wall breaking rate is high; again after alkali treatment; make Phellinus igniarius (L. ex Fr.) Quel. organizational structure more loose; be conducive to the leaching of Phellinus igniarius (L. ex Fr.) Quel. sporophore functional components, and improve the lixiviate yield of functional components.
During the invention process, comprise the steps
(1) Phellinus igniarius (L. ex Fr.) Quel. sporophore coarse powder preparation: Phellinus igniarius (L. ex Fr.) Quel. sporophore is cut to about 2cm * 2cm fritter with cutter, then pulverize with Ordinary pulverization machine, cross 10 mesh sieves, obtain coarse powder.
(2) regulate coarse powder water content: 10%～14%.
(3) Phellinus igniarius (L. ex Fr.) Quel. sporophore fine powder preparation: Phellinus igniarius (L. ex Fr.) Quel. coarse powder is put into twin (double) screw extruder feeder; regulating feeder screw speed is 40～60r/min; Phellinus igniarius (L. ex Fr.) Quel. coarse powder enters in extruder and pushes via feeder; regulate main-machine screw rotating speed 70r/min; by circulation soft water cooling system main control system temperature, be 60～80 ℃, the die head aperture of extruder discharging opening is 4～8mm
,through the above-mentioned Phellinus igniarius (L. ex Fr.) Quel. fine powder that pushes to obtain.
(4) alkali treatment: Phellinus igniarius (L. ex Fr.) Quel. fine powder is with being 0.6mol/L NaOH, and material: alkali liquor=1:5 soaks 5hr at 25 ℃, and the Phellinus igniarius (L. ex Fr.) Quel. fine powder after immersion filters and obtains filtering residue through 300 mesh filter screens, and filtering residue is washed till neutrality with deionized water, obtains Phellinus igniarius (L. ex Fr.) Quel. wet-milling, standby.
Advantage of the present invention and good effect
During the present invention adopts, warm Twin-Screw Extrusion Technology is to Phellinus igniarius (L. ex Fr.) Quel. sporophore wall breaking pulverization; obtain Phellinus igniarius (L. ex Fr.) Quel. fine powder; through alkali soak at room temperature, process, avoided high temperature, the destruction of high pressure to thermal sensitivity composition, gained powder size is fine and even more; cell wall breaking rate is high, the Phellinus igniarius (L. ex Fr.) Quel. wet-milling of short texture; changed effective ingredient dissolution characteristic, extraction process is simplified, and shortens extraction time; save the energy, and effective ingredient stripping quantity increases considerably.
The method has following some advantage
1. adopt twin screw extruding gained Phellinus igniarius (L. ex Fr.) Quel. fine powder particle diameter little
Phellinus igniarius (L. ex Fr.) Quel. fine powder is before 200 orders, be trapped part seldom, as 30 and during 40 order fine powder all filter, when 60 orders, 80 orders and 100 order, rejection is respectively 1.84%, 2.07% and 2.5%, 200 order when above, just starts to have more Phellinus igniarius (L. ex Fr.) Quel. sporophore granule to be trapped, when rejection is 25%, 250 eye mesh screen, filtration rate is still 61.5%; And the gained Phellinus igniarius (L. ex Fr.) Quel. coarse powder of Ordinary pulverization, during 60 eye mesh screen, filtration rate is only 9.15%, major part had been trapped before 60 orders, as 20 orders, 30 orders and 40 order rejection are respectively 14.58%, 39.86% and 19.44%.
2. the Phellinus igniarius (L. ex Fr.) Quel. cell breakage degree of pushing through twin screw is high
After Ordinary pulverization, particle size distribution < 60 object Phellinus igniarius (L. ex Fr.) Quel. coarse powder, under 100 times of scanning electron microscopies, unequigranular is equal, and granule footpath majority is greater than 100um, and under 5000 times of scanning electron microscopies, tube is complete; Through twin screw extruding, pulverize; particle size distribution is at 60～80 orders and < 250 object Phellinus igniarius (L. ex Fr.) Quel. fine powders; under 100 times of scanning electron microscopies; all present uniform granule; granule footpath is significantly less than 100um, under 5000 times of scanning electron microscopies, observes, and the tube majority of 60 order～80 order Phellinus igniarius (L. ex Fr.) Quel. fine powders is broken; only have the tube that is not broken of part, and cross 250 eye mesh screens can't see complete tube completely.
3. the Phellinus igniarius (L. ex Fr.) Quel. fine powder yield of extraction pushing through twin screw is than the height of Ordinary pulverization
Phellinus igniarius (L. ex Fr.) Quel. fine powder functional components extraction ratio is apparently higher than the coarse powder yield of Ordinary pulverization gained, and the extraction ratio of its polyphenol, flavone, crude polysaccharides has increased respectively 276%, 153% and 268%; And the residue yield of fine powder is lower than coarse powder, residue has reduced by 8.7%.
4. alkali treatment can further improve the lixiviate yield of functional components:
Screw extruding gained Phellinus igniarius (L. ex Fr.) Quel. fine powder is after alkali treatment, and residue yield reduces, and residue has reduced by 6.3%; And the extraction ratio of functional components polyphenol, flavone and crude polysaccharides has increased respectively 21.3%, 20.9% and 18.6%.
accompanying drawing content:
Figure
1. Phellinus igniarius (L. ex Fr.) Quel. coarse powder particle size distribution.
Fig. 2. Phellinus igniarius (L. ex Fr.) Quel. fine powder particle size distribution.
Fig. 3. screw extruding combined alkali is processed the impact on extractum and residue yield.
Fig. 4. 100 times, scanning electron microscope picture, Ordinary pulverization, < 60 orders, unequigranular is equal, and granule footpath majority is greater than 100um.
Fig. 5. 100 times, scanning electron microscope picture, screw extruding is pulverized, 60 order～80 orders, uniform particles, granule footpath is significantly less than 100um.
Fig. 6. 100 times, scanning electron microscope picture, screw extruding is pulverized, < 250 orders, uniform particles, granule footpath is significantly less than 100um.
Fig. 7. 5000 times, scanning electron microscope picture, Ordinary pulverization, < 60 orders, tube is complete.
Fig. 8. 5000 times, scanning electron microscope picture, screw extruding is pulverized, 60 order～80 orders, tube majority is broken, the tube that only has part not to be broken.
Fig. 9. 5000 times, scanning electron microscope picture, screw extruding is pulverized, and < 250 orders, can't see complete tube.
The specific embodiment
The present invention is further illustrated by the following examples.
Embodiment:
(1) Phellinus igniarius (L. ex Fr.) Quel. sporophore is first cut into the fritter of about 2cm * 2cm with cutter, with Ordinary pulverization machine, pulverizes, and crosses 12 mesh sieves, obtains coarse powder.
(2) weigh 2kg coarse powder (water content 4 ~ 10%), spray deionized water 80ml, stir even all, make coarse powder water content reach 10 ~ 14%.
(3) twin screen extrusion apparatus debugging: Phellinus igniarius (L. ex Fr.) Quel. coarse powder is put into feeder, enter in extruder and push via feeder; The rotating speed of feeder is adjusted to 40r/min before extruding starts, at the uniform velocity reinforced, and the speed that control Phellinus igniarius (L. ex Fr.) Quel. coarse powder is transported to extruder from feeder is 5～6 kgs/hour, is adjusted to the screw speed of extruder and synchronizes after extruding starts, and reaches 70r/min; In extrusion process, torque is excessive, and while reaching 20Nm, reducing rate of feeding is 50～60r/min; With circulation soft water cooling system control shear zone and extruder terminal temperature, be 60～80 ℃, the die head aperture of extruder discharging opening is 4～8mm, and last material is out squeezed by the mould mouth of extruder, obtains Phellinus igniarius (L. ex Fr.) Quel. fine powder.
(4) alkali treatment: get Phellinus igniarius (L. ex Fr.) Quel. fine powder 1kg; add 0.6mol/L NaOH solution 5kg; at 25 ℃, soak; at interval of 1hr, stir once; soak after 5hr, with 300 mesh filter screen press filtrations, obtain filtering residue, filtering residue is washed till neutrality with deionized water; obtain Phellinus igniarius (L. ex Fr.) Quel. wet-milling, this Phellinus igniarius (L. ex Fr.) Quel. wet-milling is the material that functional components extracts use.
Claims (3)
1. a kind of pre-treating method that prepared by the claimed Phellinus igniarius (L. ex Fr.) Quel. functional components of this patent, its feature 1 is: warm twin screw extrusion process in utilization, obtain grain diameter and be less than 100um, even particle distribution, cell breakage is Phellinus igniarius (L. ex Fr.) Quel. fine powder thoroughly; Its feature 2 is: gained Phellinus igniarius (L. ex Fr.) Quel. fine powder is processed through dipping by lye, is washed to neutrality, filters, and obtains the Phellinus igniarius (L. ex Fr.) Quel. fine powder (wet-milling) of short texture, then extracts to obtain Phellinus igniarius (L. ex Fr.) Quel. functional components through substep.
2. the middle temperature twin screw extrusion process in claim 1, regulating the water content of Ordinary pulverization gained Phellinus igniarius (L. ex Fr.) Quel. sporophore coarse powder is 10%～14%, via feeder, enters in extruder and pushes; Controlling shear zone and extruder terminal temperature is 60～80 ℃, and the die head aperture of extruder discharging opening is 4～8mm.
3. the immersion concentration of lye requiring in right 1 is 0.6mol/L NaOH, 25 ℃ of temperature, soak time 5hr; material: alkali liquor=1:5, the Phellinus igniarius (L. ex Fr.) Quel. fine powder after immersion filters and obtains filtering residue through 300 mesh filter screens, and filtering residue is washed till neutrality with deionized water; obtain Phellinus igniarius (L. ex Fr.) Quel. wet-milling, standby.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105250351A (en) * | 2015-10-10 | 2016-01-20 | 合肥工业大学 | Extruding wall-breaking enzymatic extraction technology of fiveleaf gynostemma herb extracting solution |
| CN105920053A (en) * | 2016-05-13 | 2016-09-07 | 孙华建 | Preparation method of phellinus igniarius fine powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105250351A (en) * | 2015-10-10 | 2016-01-20 | 合肥工业大学 | Extruding wall-breaking enzymatic extraction technology of fiveleaf gynostemma herb extracting solution |
| CN105920053A (en) * | 2016-05-13 | 2016-09-07 | 孙华建 | Preparation method of phellinus igniarius fine powder |
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Application publication date: 20140827 |